Sodium Hydroxide → 4-[N-(2-Benzyloxy-5-bromobenzyl)aminomethyl]Benzoic Acid

HRID 1106787노트

반응식

HRID 1106787 반응식
[CH2:1]([O:8][C:9]1[CH:28]=[CH:27][C:26]([Br:29])=[CH:25][C:10]=1[CH2:11][NH:12][CH2:13][C:14]1[CH:24]=[CH:23][C:17]([C:18]([O:20]CC)=[O:19])=[CH:16][CH:15]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>CO>[CH2:1]([O:8][C:9]1[CH:28]=[CH:27][C:26]([Br:29])=[CH:25][C:10]=1[CH2:11][NH:12][CH2:13][C:14]1[CH:24]=[CH:23][C:17]([C:18]([OH:20])=[O:19])=[CH:16][CH:15]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22675503ethyl 4-[N-(2-benzyloxy-5-bromobenzyl)aminomethyl]benzoate

생성물 1

HCID 47205174-[N-(2-Benzyloxy-5-bromobenzyl)aminomethyl]Benzoic Acid수율 60.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a mixture of ethyl 4-[N-(2-benzyloxy-5-bromobenzyl)-aminomethyl]benzoate (1.4 g) in methanol (25 ml) was added 2N sodium hydroxide solution (7.7 ml). The mixture was heated at reflux for 30 minutes, left to stand for 2 hours at ambient temperature, the solvent evaporated and the residue mixed with water (20 ml). The mixture was acidified with acetic acid, the precipitate filtered off and crystallised form ethyl acetate to give the title compound (800 mg) mpt 209° C. The starting material was prepared as follows:

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 30 minutes
  3. waitleft
  4. customthe solvent evaporated
  5. additionthe residue mixed with water (20 ml)
  6. filtrationthe precipitate filtered off
  7. customcrystallised
  8. customform ethyl acetate

출처 및 근거

ORD 기록
ord-ec3d0ba5fe944f74800dc8c14970af68
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06057345

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